CN104849366A - Detection system and detection method - Google Patents
Detection system and detection method Download PDFInfo
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- CN104849366A CN104849366A CN201510236831.3A CN201510236831A CN104849366A CN 104849366 A CN104849366 A CN 104849366A CN 201510236831 A CN201510236831 A CN 201510236831A CN 104849366 A CN104849366 A CN 104849366A
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Abstract
The invention provides a detection system and a detection method. The detection system comprises a hydrogen supply device, an inert gas supply device, a vaporization chamber and a gas mixing chamber, wherein the vaporization chamber is provided with a sample inlet for introducing chlorosilane, a first inlet of the gas mixing chamber is communicated with an outlet of the vaporization chamber, and an outlet of the hydrogen supply device is connected with an outlet of the inert gas supply device in parallel and is connected to a second inlet of the mixing chamber; and the detection system also comprises a chlorosilane reduction device, a removal device, a methane adsorption and desorption device, a gas phase chromatograph and a data output device, which are sequentially connected with one another in series, an inlet of the chlorosilane reduction device is communicated with the outlet of the gas mixing chamber, and the removal device is used for removing hydrogen chloride and unreacted chlorosilane. Carbon element in the chlorine-containing silane is reduced by the chlorosilane reduction device to methane, then the methane is sent into the gas phase chromatograph, and the content of the carbon in the methane is determined, so that the total carbon content in the chlorosilane can be detected.
Description
Technical field
The present invention relates to analysis detection field, in particular to a kind of detection system and detection method.
Background technology
In current polysilicon preparation field, when producing trichlorosilane, association silicon tetrachloride, dichlorosilane can be produced.That is, in polysilicon preparation field, three kinds of chlorosilanes can not be produced separately, but three kinds of chlorosilanes exist (chlorine-containing silane namely in the present invention) simultaneously.Wherein, trichlorosilane is the important raw and processed materials preparing grade multi-crystalline silicon and solar-grade polysilicon, is also the important intermediate manufacturing silane coupling agent and other organosilicon product.Along with international and domestic to the increase day by day of polysilicon demand, the stable supply of in enormous quantities and high-quality trichlorosilane just seems and of crucial importance.
At present, usually adopt distillation technology to purify to trichlorosilane in chlorine-containing silane, impurity content is more low better, and wherein said impurity comprises the carbon (total carbon) that various forms exists.In the quality index of polysilicon, carbon content is an important index.Carbon content number directly affect polycrystalline silicon material application and device efficiency, the carbon in chlorine-containing silane is then the important sources of carbon in polysilicon, therefore for the measurement of total carbon content in chlorine-containing silane, seems particularly important.
The existence form of the carbon mainly carbon compound such as various methyl chlorosilane, ethyl chlorosilane, methenyl choloride in chlorine-containing silane.Because chlorosilane boiling point is low, inflammable, explosive, facile hydrolysis, then produces hydrogen chloride and hydrated SiO 2 after hydrolysis, makes system corrosion, blocking and contaminated, so very difficult to the on-line checkingi analysis of chlorosilane.At present, for carbon content in chlorosilane, the instrument such as gas chromatographicanalyzer, infrared spectrum analyser, gas-matter analyser is generally adopted to carry out analysis to measure.Although above analytical equipment can be carried out carbon content in chlorosilane, all can only carry out analysis to single or fractions and detect, and the total carbon content in chlorosilane can not be measured.Therefore, adopt existing method of testing, Monitoring and Controlling can not be carried out to carbon content in these intermediate product of trichlorosilane, thus the total carbon also just can not monitored in chlorosilane is on the impact of polysilicon product quality.High-temperature hydrogen reduction gas chromatograph is used for surveying the element such as phosphorus, arsenic in trichlorosilane once in a while, but is never used to measure total carbon content, and also not relevant method adopts this equipment to measure the total carbon content in chlorine-containing silane.
Summary of the invention
Fundamental purpose of the present invention is to provide a kind of detection system and detection method, to detect the total carbon content in chlorine-containing silane.
To achieve these goals, according to an aspect of the present invention, provide a kind of detection system, for detecting the total carbon content in chlorine-containing silane, this detection system comprises hydrogen feeding mechanism, inert gas feeding mechanism, vaporizer and mixing chamber, vaporizer has the injection port for passing into chlorosilane, and the first entrance of mixing chamber is connected with the outlet of vaporizer, and the outlet of hydrogen feeding mechanism and the outlet of inert gas feeding mechanism are connected in parallel in the second entrance of mixing chamber; This detection system also comprise be arranged in series successively chlorosilane reduction apparatus, remove device, methane adsorption desorption device, gas chromatograph and data output device, and the entrance of chlorosilane reduction apparatus and the outlet of mixing chamber, remove device for removing hydrogen chloride and unreacted chlorosilane.
Further, detection system also comprises exhausting pipeline, and removes the outlet of device, the entrance of methane adsorption desorption device, the outlet of inert gas feeding mechanism, the entrance of gas chromatograph, the outlet of methane adsorption desorption device and exhausting pipeline and be linked in sequence on six-way valve; When six-way valve is adjusted to Enrichment Mode, remove between the outlet of device and the entrance of methane adsorption desorption device, between the outlet of inert gas feeding mechanism and the entrance of gas chromatograph and conducting between the outlet of methane adsorption desorption device and exhausting pipeline; When six-way valve is adjusted to analytical model, remove between the outlet of device and exhausting pipeline, between the entrance of methane adsorption desorption device and the outlet of inert gas feeding mechanism, conducting between the outlet of methane adsorption desorption device and the entrance of gas chromatograph.
Further, the outlet of inert gas feeding mechanism, between the outlet of hydrogen feeding mechanism and the second entrance, T-valve is provided with.
Further, chlorosilane reduction apparatus comprises quartz ampoule and well heater.
Further, remove device and comprise the hydrogen chloride connected successively and remove pipe and condenser, condenser comprises the condensing container filling liquid nitrogen and the dehydrating tube being placed in liquid nitrogen.
Further, methane adsorption desorption device comprises the adsorption desorption container filling solvent and the enriching column be arranged in solvent; When methane adsorption desorption device is used for adsorbed methane, solvent is liquid nitrogen, and when methane adsorption desorption device is used for desorption methane, solvent is boiling water.
Further, hydrogen feeding mechanism comprises sources of hydrogen and the hydrogen that is connected with sources of hydrogen reduces pressure pressure regulator; Inert gas feeding mechanism comprises inert gas source and the inert gas that is connected with inert gas source reduces pressure pressure regulator; Gas chromatograph comprises flame ionization ditector; Data output device is computer or data recorder.
To achieve these goals, according to another aspect of the present invention, provide a kind of detection method, this detection method utilizes the bright detection system provided of this law to detect the total carbon content in chlorine-containing silane, this detection method comprises the following steps: step S1, the inert gas feeding mechanism opened in detection system, uses inert gas to carry out gas displacement to detection system; Step S2, the chlorosilane reduction apparatus in detection system is warming up to preset temperature; Step S3, hydrogen feeding mechanism, gas chromatograph and the data output device opened in detection system, and hydrogen is passed in detection system; Step S4, pass into chlorosilane to the injection port in detection system, make the chlorosilane reduction apparatus reaction in the detection system of chlorosilane and hydrogen form methane; Step S5, utilize the methane adsorption desorption device in detection system to carry out adsorption and desorption to methane, and utilize gas chromatograph to carry out parsing test to the methane after desorption, adopt the peak area of data output device record methane simultaneously.
Further, inert gas feeding mechanism comprises inert gas decompression pressure regulator, is provided with T-valve between the second entrance of the mixing chamber in the outlet of inert gas feeding mechanism, the outlet of hydrogen feeding mechanism and detection system; In step S1, regulate inert gas decompression pressure regulator to 1 ~ 5MPa, and swivel tee valve is to make inert gas to the gas displacement 3 ~ 10min in detection system.
Further, in detection system remove device comprise the hydrogen chloride connected successively remove pipe and condenser, detection system also comprises six-way valve, and methane adsorption desorption device comprises enriching column; In step S2, inserted by dehydrating tube in liquid nitrogen, six-way valve is adjusted to analytical model, then chlorosilane reduction apparatus is warming up to 800 ~ 1100 DEG C, the heating-up time is 40 ~ 60min.
Further, hydrogen feeding mechanism comprises sources of hydrogen and the hydrogen that is connected with sources of hydrogen reduces pressure pressure regulator, gas chromatograph comprises flame ionization ditector; In step S3, open sources of hydrogen, and swivel tee revolves and makes hydrogen enter detection system, then gas chromatograph is opened, to gas chromatograph, injector temperature is 80 ~ 120 DEG C, the temperature of chromatographic column 180 ~ 200 DEG C, the temperature of detecting device is 200 ~ 250 DEG C, the nebulizer gas pressure of gas chromatograph is 0.395 ~ 0.405MPa, in gas chromatograph, the flow of hydrogen is 30ml/min ~ 50ml/min, and control hydrogen decompression pressure regulator make Hydrogen Vapor Pressure control, at 2.0Mpa, finally light flame ionization ditector and start data output device.
Further, in step S4, rotate six-way valve to Enrichment Mode, enriching column is inserted in liquid nitrogen simultaneously, the chlorosilane then utilizing microsyringe to draw 20 ~ 100 microlitres enters the vaporizer in detection system.
Further, in step S5, after passing into chlorosilane 10 ~ 20min to the injection port in detection system, rotate six-way valve to analytical model, enriching column is inserted in boiling water and carries out parsing test, simultaneously by the peak area of data output device record methane; After step s 5, detection method also comprises: enriching column is taken out from boiling water, and swivel tee valve is lowered the temperature to chlorosilane reduction apparatus to pass into inert gas; Close hydrogen feeding mechanism and data output device, and close inert gas feeding mechanism when chlorosilane reduction apparatus is cooled to below 200 DEG C.
Further, chlorine-containing silane is formed by the raw material reaction comprising hydrogen and tetrachloro silicane, and the key component of chlorine-containing silane is dichlorosilane, trichlorosilane and silicon tetrachloride.
Apply technical scheme of the present invention, carbon hydro-reduction in chlorine-containing silane is methane by chlorosilane reduction apparatus by the present invention, then methane to be sent in gas chromatograph and the carbon content in methane is measured, thus achieving the total carbon content detected in chlorine-containing silane.
Accompanying drawing explanation
The Figure of description forming a application's part is used to provide a further understanding of the present invention, and schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 shows the schematic diagram of the detection system provided according to the specific embodiment of the invention; And
Fig. 2 a six-way valve shown in the detection system provided according to the specific embodiment of the invention is adjusted to schematic diagram during Enrichment Mode; And
Fig. 2 b six-way valve shown in the detection system provided according to the specific embodiment of the invention is adjusted to schematic diagram during analytical model.
Embodiment
It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can combine mutually.Below with reference to the accompanying drawings and describe the application in detail in conjunction with the embodiments.
It should be noted that used term is only to describe embodiment here, and be not intended to the illustrative embodiments of restricted root according to the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative is also intended to comprise plural form, in addition, it is to be further understood that, " comprise " when using term in this manual and/or " comprising " time, it indicates existing characteristics, step, operation, device, assembly and/or their combination.
For convenience of description, here can usage space relative terms, as " ... on ", " in ... top ", " at ... upper surface ", " above " etc., be used for the spatial relation described as a device shown in the figure or feature and other devices or feature.Should be understood that, space relative terms is intended to comprise the different azimuth in use or operation except the described in the drawings orientation of device.Such as, " in other devices or structure below " or " under other devices or structure " will be positioned as after if the device in accompanying drawing is squeezed, being then described as the device of " above other devices or structure " or " on other devices or structure ".Thus, exemplary term " in ... top " can comprise " in ... top " and " in ... below " two kinds of orientation.This device also can other different modes location (90-degree rotation or be in other orientation), and relatively describe space used here and make respective explanations.
From background technology, prior art cannot measure the total carbon content in chlorine-containing silane.The present inventor studies for the problems referred to above, provides a kind of detection system, for detecting the total carbon content in chlorine-containing silane.As shown in Figure 1, this detection system comprises: hydrogen feeding mechanism 1, inert gas feeding mechanism 2, vaporizer 3 and mixing chamber 4, vaporizer 3 has the injection port for passing into chlorosilane, first entrance of mixing chamber 4 is connected with the outlet of vaporizer 3, and the outlet of hydrogen feeding mechanism 1 and the outlet of inert gas feeding mechanism 2 are connected in parallel in the second entrance of mixing chamber 4; This detection system also comprise be arranged in series successively chlorosilane reduction apparatus 6, remove device, methane adsorption desorption device, gas chromatograph 12 and data output device 13, and the outlet of the entrance of chlorosilane reduction apparatus 6 and mixing chamber 4, remove device for removing hydrogen chloride and unreacted chlorosilane.
Carbon hydro-reduction in chlorine-containing silane is methane by chlorosilane reduction apparatus 6 by above-mentioned detection device, then to be sent into by methane in gas chromatograph 12 and to measure the carbon content in methane, thus achieving the total carbon content detected in chlorine-containing silane.
In a preferred embodiment, detection system also comprises exhausting pipeline, and removes the outlet of device, the entrance of methane adsorption desorption device, the outlet of inert gas feeding mechanism 2, the entrance of gas chromatograph 12, the outlet of methane adsorption desorption device and exhausting pipeline and be linked in sequence on six-way valve 9; When six-way valve 9 is adjusted to Enrichment Mode, remove between the outlet of device and the entrance of methane adsorption desorption device, between the outlet of inert gas feeding mechanism 2 and the entrance of gas chromatograph 12 and conducting (as shown in Figure 2 a) between the outlet of methane adsorption desorption device and exhausting pipeline; When six-way valve 9 is adjusted to analytical model, remove between the outlet of device and exhausting pipeline, between the entrance of methane adsorption desorption device and the outlet of inert gas feeding mechanism 2, conducting (as shown in Figure 2 b) between the outlet of methane adsorption desorption device and the entrance of gas chromatograph 12.
Preferably, the outlet of inert gas feeding mechanism 2, between the outlet of hydrogen feeding mechanism 1 and the second entrance, T-valve 5 is provided with.Chlorosilane reduction apparatus 6 comprises quartz ampoule and well heater.Remove device to comprise the hydrogen chloride connected successively and remove pipe 7 and condenser, condenser comprises the condensing container filling liquid nitrogen and the dehydrating tube 8 being placed in liquid nitrogen.
Particularly, methane adsorption desorption device comprises the adsorption desorption container filling solvent and the enriching column 10 be arranged in solvent; When methane adsorption desorption device is used for adsorbed methane, solvent is liquid nitrogen, and when methane adsorption desorption device is used for desorption methane, solvent is boiling water.Hydrogen feeding mechanism 1 comprises sources of hydrogen and the hydrogen that is connected with sources of hydrogen reduces pressure pressure regulator; Inert gas feeding mechanism 2 comprises inert gas source and the inert gas that is connected with inert gas source reduces pressure pressure regulator; Gas chromatograph 12 comprises flame ionization ditector; Data output device 13 is computer or data recorder.Preferably, inert gas is nitrogen.
Wherein, flame ionization ditector (FID) detects widely used a kind of detecting device in analysis design mothod at gas chromatograph 12, its principle of work is: produce flame for the energy with oxygen combustion in hydrogen and air, when detected sample enters flame, under the high energy effect of flame, be excited and produce ion.Ion, under the effect of interpolar DC electric field, is excited and produces ion.Ion with regard to displacement, defines a kind of weak current under the effect of interpolar DC electric field, then flows through high resistance and takes out voltage signal, send into secondary signal recorder and go on record after amplifying.
According to another aspect of the present invention, provide a kind of detection method, this detection method utilizes the bright detection system provided of this law to detect the total carbon content in chlorine-containing silane, this detection method comprises the following steps: step S1, the inert gas feeding mechanism 2 opened in detection system, uses inert gas to carry out gas displacement to detection system; Step S2, the chlorosilane reduction apparatus 6 in detection system is warming up to preset temperature; Step S3, the hydrogen feeding mechanism 1 opened in detection system, gas chromatograph 12 and data output device 13, and hydrogen is passed in detection system; Step S4, pass into chlorosilane to the injection port in detection system, chlorosilane and hydrogen chlorosilane reduction apparatus 6 is in the detection system reacted and forms methane; Step S5, utilize the methane adsorption desorption device in detection system to carry out adsorption and desorption to methane, and utilize the methane after gas chromatograph 12 pairs of desorptions to carry out parsing test, adopt data output device 13 to record the peak area of methane simultaneously.Wherein, chlorine-containing silane is formed by the raw material reaction comprising hydrogen and tetrachloro silicane, and the key component of chlorine-containing silane is dichlorosilane, trichlorosilane and silicon tetrachloride.
Illustrative embodiments according to detection method provided by the invention will be described in more detail below.But these illustrative embodiments can be implemented by multiple different form, and should not be interpreted as being only limited to embodiment set forth herein.Should be understood that, provide these embodiments be in order to make the application open thorough and complete, and the design of these illustrative embodiments is fully conveyed to those of ordinary skill in the art.
First, perform step S1, namely open the inert gas feeding mechanism 2 in detection system, use inert gas to carry out gas displacement to detection system.Preferably, inert gas feeding mechanism 2 comprises inert gas decompression pressure regulator, is provided with T-valve 5 between the second entrance of the mixing chamber 4 in the outlet of inert gas feeding mechanism 2, the outlet of hydrogen feeding mechanism 1 and detection system; In step S1, regulate inert gas decompression pressure regulator to 1 ~ 5MPa, and swivel tee valve 5 is to make inert gas to the gas displacement 3 ~ 10min in detection system.
Then, perform step S2, be warming up to preset temperature by the chlorosilane reduction apparatus 6 in detection system.Preferably, the device that removes in detection system comprises the hydrogen chloride connected successively and removes pipe 7 and condenser, and detection system also comprises six-way valve 9, and methane adsorption desorption device comprises enriching column 10; In step S2, insert in liquid nitrogen by dehydrating tube 8, six-way valve 9 is adjusted to analytical model, then chlorosilane reduction apparatus 6 is warming up to 800 ~ 1100 DEG C, the heating-up time is 40 ~ 60min.
Next, perform step S3, namely open the hydrogen feeding mechanism 1 in detection system, gas chromatograph 12 and data output device 13, and pass into hydrogen in detection system.When hydrogen feeding mechanism 1 comprises sources of hydrogen and the hydrogen that is connected with sources of hydrogen reduces pressure pressure regulator, gas chromatograph 12 comprises flame ionization ditector; In step S3, open sources of hydrogen, and swivel tee revolves and makes hydrogen enter detection system, then gas chromatograph 12 is opened, to gas chromatograph 12, injector temperature is 80 ~ 120 DEG C, the temperature of chromatographic column 180 ~ 200 DEG C, the temperature of detecting device is 200 ~ 250 DEG C, the nebulizer gas pressure of gas chromatograph 12 is 0.395 ~ 0.405MPa, in gas chromatograph 12, the flow of hydrogen is 30ml/min ~ 50ml/min, and control hydrogen decompression pressure regulator make Hydrogen Vapor Pressure control at 2.0Mpa, finally light flame ionization ditector and start data output device 13.
Next, perform step S4, namely pass into chlorosilane to the injection port in detection system, chlorosilane and hydrogen chlorosilane reduction apparatus 6 is in the detection system reacted and forms methane.Particularly, in step S4, rotate to Enrichment Mode by six-way valve 9, enriching column 10 is inserted in liquid nitrogen simultaneously, the chlorosilane then utilizing microsyringe to draw 20 ~ 100 microlitres enters the vaporizer 3 in detection system.
Finally, perform step S5, namely utilize the methane adsorption desorption device in detection system to carry out adsorption and desorption to methane, and utilize the methane after gas chromatograph 12 pairs of desorptions to carry out parsing test, adopt data output device 13 to record the peak area of methane simultaneously.Particularly, in step S5, after passing into chlorosilane 10 ~ 20min to the injection port in detection system, rotate six-way valve 9 to analytical model, enriching column 10 is inserted in boiling water and carries out parsing test, recorded the peak area of methane simultaneously by data output device 13; After step s 5, detection method also comprises: enriching column 10 is taken out from boiling water, and swivel tee valve 5 is lowered the temperature to chlorosilane reduction apparatus 6 to pass into inert gas; Close hydrogen feeding mechanism 1 and data output device 13, and close inert gas feeding mechanism 2 when chlorosilane reduction apparatus 6 is cooled to below 200 DEG C.
Detection system provided by the invention and detection method is further illustrated below in conjunction with concrete steps.
In this detection method, using nitrogen as inert gas, its concrete implementation step is as follows:
1. open Nitrogen source gases, regulate nitrogen decompression pressure regulator to 2.0MPa; Swivel tee valve is to " nitrogen " position.Nitrogen displacement 5min is carried out to system;
2. dehydrating tube is inserted in liquid nitrogen, six-way valve is adjusted to " analysis " position;
3. the reduction temperature setting quartz ampoule is 800 ~ 1200 DEG C, and the temperature-rise period time is 40 ~ 60min, heats quartz ampoule;
4. after temperature reaches, open sources of hydrogen, T-valve is rotated to " hydrogen " position, makes hydrogen enter in mixing chamber and subsequent instrumentation;
5. be communicated with the gas circuit of gas chromatograph, open gas chromatograph; When the parameter such as temperature, pressure, flow of gas chromatograph, in normal range, (namely in gas chromatograph, injector temperature is 80 ~ 120 DEG C, the temperature of chromatographic column 180 ~ 200 DEG C, the temperature of detecting device is 200 ~ 250 DEG C, nebulizer gas pressure is 0.395 ~ 0.405MPa, the flow of hydrogen is 30ml/min ~ 50ml/min), then control hydrogen decompression pressure regulator and make total hydrogen pressure control at 2.0Mpa;
6. light the fid detector of gas chromatograph, and start computer record program and data processor;
7. six-way valve is rotated to Enrichment Mode, enriching column is inserted in liquid nitrogen simultaneously;
8. the sample of 20 ~ 100 microlitre chlorosilane determination content carbons is drawn with dry microsyringe, and standard model, from vaporizer; Injection port inject, start to clock simultaneously;
9. after 10 ~ 20min, rotate six-way valve to analytical model, enriching column is inserted in boiling water simultaneously and resolve test;
10. detected the peak area of methane by the program software record in computer, calculate the response of standard model;
11. continuous strands are advanced sample at least 2 times, until response relative deviation is less than 5%, average, standard model is completed;
12. draw 20 ~ 100 microlitre chlorosilane samples with microscale sampler, and repeat step 8 ~ step 11, the response of combined standard sample and content, calculate total carbon content in sample;
13. end of operations, enriching column; From boiling water; In take out; By T-valve; Be threaded to " nitrogen " position, lower the temperature to quartz ampoule; Close sources of hydrogen; Close computer record program and data processor; Liquid nitrogen is refunded in liquid nitrogen biological container and preserves; When furnace tube temperature is down to less than 200 DEG C, close source nitrogen.
As can be seen from the above embodiments, the above-mentioned example of the present invention achieves following technique effect: the carbon hydro-reduction in chlorine-containing silane is methane by chlorosilane reduction apparatus by the present invention, then methane to be sent in gas chromatograph and the carbon content in methane is measured, thus achieving the total carbon content detected in chlorine-containing silane.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (14)
1. a detection system, for detecting the total carbon content in chlorine-containing silane, is characterized in that,
Described detection system comprises hydrogen feeding mechanism, inert gas feeding mechanism, vaporizer (3) and mixing chamber (4), described vaporizer (3) has the injection port for passing into chlorosilane, first entrance of described mixing chamber (4) is connected with the outlet of described vaporizer (3), and the outlet of described hydrogen feeding mechanism and the outlet of described inert gas feeding mechanism are connected in parallel in the second entrance of described mixing chamber (4);
Described detection system also comprise be arranged in series successively chlorosilane reduction apparatus (6), remove device, methane adsorption desorption device, gas chromatograph (12) and data output device (13), and the entrance of described chlorosilane reduction apparatus (6) and the outlet of described mixing chamber (4), described in remove device for removing hydrogen chloride and unreacted described chlorosilane.
2. detection system according to claim 1, it is characterized in that, described detection system also comprises exhausting pipeline, and described in remove the outlet of device, the entrance of described methane adsorption desorption device, the outlet of described inert gas feeding mechanism, the entrance of described gas chromatograph (12), the outlet of described methane adsorption desorption device and described exhausting pipeline and be linked in sequence on six-way valve (9); When described six-way valve (9) is adjusted to Enrichment Mode, described in remove between the outlet of device and the entrance of described methane adsorption desorption device, between the outlet of described inert gas feeding mechanism and the entrance of described gas chromatograph (12) and conducting between the outlet of described methane adsorption desorption device and described exhausting pipeline; When described six-way valve (9) is adjusted to analytical model, described in remove between the outlet of device and described exhausting pipeline, between the entrance of described methane adsorption desorption device and the outlet of described inert gas feeding mechanism, conducting between the outlet of described methane adsorption desorption device and the entrance of described gas chromatograph (12).
3. detection system according to claim 1, is characterized in that, the outlet of described inert gas feeding mechanism, is provided with T-valve (5) between the outlet of described hydrogen feeding mechanism and described second entrance.
4. detection system according to claim 1, is characterized in that, described chlorosilane reduction apparatus (6) comprises quartz ampoule and well heater.
5. detection system according to claim 1, it is characterized in that, the described device that removes comprises the hydrogen chloride connected successively and removes pipe (7) and condenser, and described condenser comprises the condensing container filling liquid nitrogen and the dehydrating tube (8) being placed in described liquid nitrogen.
6. detection system according to claim 1, is characterized in that, described methane adsorption desorption device comprises the adsorption desorption container filling solvent and the enriching column (10) be arranged in described solvent; When described methane adsorption desorption device is used for adsorbed methane, described solvent is liquid nitrogen, and when described methane adsorption desorption device is used for desorption methane, described solvent is boiling water.
7. detection system according to claim 1, is characterized in that, described hydrogen feeding mechanism comprises sources of hydrogen and the hydrogen that is connected with described sources of hydrogen reduces pressure pressure regulator (1); Described inert gas feeding mechanism comprises inert gas source and the inert gas that is connected with described inert gas source reduces pressure pressure regulator (2); Described gas chromatograph (12) comprises flame ionization ditector; Described data output device (13) is computer or data recorder.
8. a detection method, is characterized in that, described detection method utilizes the detection system according to any one of claim 1 to 10 to detect the total carbon content in chlorine-containing silane, and described detection method comprises the following steps:
Step S1, the inert gas feeding mechanism opened in described detection system, use inert gas to carry out gas displacement to described detection system;
Step S2, the chlorosilane reduction apparatus (6) in described detection system is warming up to preset temperature;
Step S3, the hydrogen feeding mechanism opened in described detection system, gas chromatograph (12) and data output device (13), and hydrogen is passed in described detection system;
Step S4, pass into chlorosilane to the injection port in described detection system, make chlorosilane reduction apparatus (6) reaction in described detection system of described chlorosilane and described hydrogen form methane;
Step S5, the methane adsorption desorption device in described detection system is utilized to carry out adsorption and desorption to described methane, and utilize described gas chromatograph (12) to carry out parsing test to the described methane after desorption, adopt described data output device (13) to record the peak area of described methane simultaneously.
9. detection method according to claim 8, is characterized in that,
Described inert gas feeding mechanism comprises inert gas decompression pressure regulator (2), is provided with T-valve (5) between the second entrance of the mixing chamber (4) in the outlet of described inert gas feeding mechanism, the outlet of described hydrogen feeding mechanism and described detection system;
In described step S1, regulate described inert gas to reduce pressure pressure regulator (2) to 1 ~ 5MPa, and rotate described T-valve (5) to make described inert gas to the gas displacement 3 ~ 10min in described detection system.
10. detection method according to claim 9, is characterized in that,
The device that removes in described detection system comprises the hydrogen chloride connected successively and removes pipe (7) and condenser, and described detection system also comprises six-way valve (9), and described methane adsorption desorption device comprises enriching column (10);
In described step S2, described dehydrating tube (8) is inserted in described liquid nitrogen, described six-way valve (9) is adjusted to analytical model, and then described chlorosilane reduction apparatus (6) is warming up to 800 ~ 1100 DEG C, the heating-up time is 40 ~ 60min.
11. detection methods according to claim 9, is characterized in that,
Described hydrogen feeding mechanism comprises sources of hydrogen and the hydrogen that is connected with described sources of hydrogen reduces pressure pressure regulator (1), described gas chromatograph (12) comprises flame ionization ditector;
In described step S3, open described sources of hydrogen, and rotate described threeway and revolve and make hydrogen enter described detection system, then described gas chromatograph (12) is opened, to described gas chromatograph (12), injector temperature is 80 ~ 120 DEG C, the temperature of chromatographic column 180 ~ 200 DEG C, the temperature of detecting device is 200 ~ 250 DEG C, the nebulizer gas pressure of described gas chromatograph (12) is 0.395 ~ 0.405MPa, described in described gas chromatograph (12), the flow of hydrogen is 30ml/min ~ 50ml/min, and control described hydrogen decompression pressure regulator (1) make Hydrogen Vapor Pressure control at 2.0Mpa, finally light described flame ionization ditector and start described data output device (13).
12. detection methods according to claim 10, it is characterized in that, in described step S4, described six-way valve (9) is rotated to Enrichment Mode, described enriching column (10) is inserted in liquid nitrogen, the described chlorosilane then utilizing microsyringe to draw 20 ~ 100 microlitres enters the vaporizer (3) in described detection system simultaneously.
13. detection methods according to claim 10, is characterized in that,
In described step S5, after passing into described chlorosilane 10 ~ 20min to the injection port in described detection system, rotate described six-way valve (9) to analytical model, described enriching column (10) is inserted in boiling water and carries out parsing test, recorded the peak area of described methane simultaneously by described data output device (13);
After described step S5, described detection method also comprises: described enriching column (10) is taken out from boiling water, rotates described T-valve (5) and lowers the temperature to described chlorosilane reduction apparatus (6) to pass into inert gas; Close described hydrogen feeding mechanism and data output device (13), and close inert gas feeding mechanism when described chlorosilane reduction apparatus (6) is cooled to below 200 DEG C.
14. detection methods according to claim 8, is characterized in that, described chlorine-containing silane is formed by the raw material reaction comprising hydrogen and tetrachloro silicane, and the key component of described chlorine-containing silane is dichlorosilane, trichlorosilane and silicon tetrachloride.
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| CN108414836A (en) * | 2018-04-27 | 2018-08-17 | 河南理工大学 | Nitrogen is gas displacing coal-bed to use complex resistance measuring system and method |
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| CN113533600B (en) * | 2021-08-09 | 2022-02-22 | 江苏鑫华半导体材料科技有限公司 | Trichlorosilane detection pretreatment method and trichlorosilane detection method |
| CN117110527A (en) * | 2023-10-25 | 2023-11-24 | 是高(北京)智能科技有限公司 | On-line detection and analysis method and system for chlorosilane impurity elements |
| CN117110527B (en) * | 2023-10-25 | 2023-12-19 | 是高(北京)智能科技有限公司 | On-line detection and analysis method and system for chlorosilane impurity elements |
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